US5948854A - Alkoxy-functional RTV compositions with increased green strength and increased storage stability - Google Patents
Alkoxy-functional RTV compositions with increased green strength and increased storage stability Download PDFInfo
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- US5948854A US5948854A US08/937,525 US93752597A US5948854A US 5948854 A US5948854 A US 5948854A US 93752597 A US93752597 A US 93752597A US 5948854 A US5948854 A US 5948854A
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- 239000000203 mixture Substances 0.000 title claims abstract description 99
- 238000003860 storage Methods 0.000 title abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 42
- 229920000642 polymer Polymers 0.000 claims abstract description 32
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- -1 amyloxy groups Chemical group 0.000 claims abstract description 26
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 19
- 125000005370 alkoxysilyl group Chemical group 0.000 claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 29
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 22
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 21
- 125000004432 carbon atom Chemical group C* 0.000 claims description 18
- 239000004215 Carbon black (E152) Substances 0.000 claims description 17
- 229930195733 hydrocarbon Natural products 0.000 claims description 17
- 125000000217 alkyl group Chemical group 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 13
- 125000001931 aliphatic group Chemical group 0.000 claims description 10
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 229920002554 vinyl polymer Chemical group 0.000 claims description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 5
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000003014 reinforcing effect Effects 0.000 claims description 5
- 125000002947 alkylene group Chemical group 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 3
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 3
- 101100177155 Arabidopsis thaliana HAC1 gene Proteins 0.000 claims 1
- 101100434170 Oryza sativa subsp. japonica ACR2.1 gene Proteins 0.000 claims 1
- 101100434171 Oryza sativa subsp. japonica ACR2.2 gene Proteins 0.000 claims 1
- 239000010936 titanium Substances 0.000 description 25
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 22
- 229910052719 titanium Inorganic materials 0.000 description 22
- 239000004615 ingredient Substances 0.000 description 15
- 239000000565 sealant Substances 0.000 description 12
- 239000002318 adhesion promoter Substances 0.000 description 9
- 235000010216 calcium carbonate Nutrition 0.000 description 9
- 238000000518 rheometry Methods 0.000 description 9
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 8
- 239000000654 additive Substances 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 6
- 229910000077 silane Inorganic materials 0.000 description 6
- 239000004590 silicone sealant Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 229920002959 polymer blend Polymers 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003138 primary alcohols Chemical class 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 150000003333 secondary alcohols Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 150000003609 titanium compounds Chemical class 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 239000004890 Hydrophobing Agent Substances 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 101150108015 STR6 gene Proteins 0.000 description 1
- 101100386054 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) CYS3 gene Proteins 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- UWGJCHRFALXDAR-UHFFFAOYSA-N diethoxy-ethyl-methylsilane Chemical compound CCO[Si](C)(CC)OCC UWGJCHRFALXDAR-UHFFFAOYSA-N 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XGZNHFPFJRZBBT-UHFFFAOYSA-N ethanol;titanium Chemical compound [Ti].CCO.CCO.CCO.CCO XGZNHFPFJRZBBT-UHFFFAOYSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003707 hexyloxy group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])O* 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- ZEIWWVGGEOHESL-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC.OC.OC.OC ZEIWWVGGEOHESL-UHFFFAOYSA-N 0.000 description 1
- 235000019645 odor Nutrition 0.000 description 1
- 125000005702 oxyalkylene group Chemical group 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000019612 pigmentation Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- UQMGAWUIVYDWBP-UHFFFAOYSA-N silyl acetate Chemical class CC(=O)O[SiH3] UQMGAWUIVYDWBP-UHFFFAOYSA-N 0.000 description 1
- 101150035983 str1 gene Proteins 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/057—Metal alcoholates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/14—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/24—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen halogen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
Definitions
- This invention relates to alkoxy-functional room temperature vulcanizing (RTV) compositions, curable in the presence of moisture, comprising polymers containing on average at least 1.2 alkoxysilyl chain terminations per molecule, a tetraalkoxytitanium compound containing on average greater than 90 mole percent of the alkoxy groups as tertiary amyloxy groups, a filler, and an alkoxysilane.
- RTV room temperature vulcanizing
- compositions which cure to elastomeric materials at room temperature are well known.
- Such compositions can be obtained by mixing polydiorganosiloxanes having reactive groups, such as silanol groups, with silane crosslinking agents, for example, alkoxysilanes, acetoxysilanes, oximosilanes, or aminosilanes.
- silane crosslinking agents for example, alkoxysilanes, acetoxysilanes, oximosilanes, or aminosilanes.
- Compositions comprising these ingredients can then be cured by exposure to atmospheric moisture at room temperature.
- Moisture curable compositions are well known for their use as sealants.
- sealants which can quickly develop green strength so that elements of a construction can be formed and will maintain the desired configuration even if handled, packaged, and shipped after relatively short cure times, without showing permanent deformation.
- Sealant compositions which can quickly develop green strength include silicone sealant compositions which evolve acetic acid, ketoximes, or amines as by-products during cure. These by-products have unpleasant odors and may corrode sensitive metals or plastics. The use of other compositions which would not have these properties would therefore be beneficial.
- One potential alternative to these compositions is an alkoxy-functional RTV composition containing tetraalkoxytitanium compounds derived from primary or secondary alcohols and liberating alcohol during cure.
- the alkoxy-functional RTV compositions containing these tetraalkoxytitanium compounds derived from primary or secondary alcohols do not have sufficient green strength for applications requiring packing and shipping of assembled components soon after manufacture.
- alkoxy-functional RTV compositions have improved green strength upon curing and improved storage stability when on average greater than 90 mole percent of the alkoxy groups of the tetraalkoxytitanium compound are tertiary-amyloxy (t-amyloxy) groups and the components are added in amounts to satisfy defined molar ratios.
- green strength as defined herein means a high-modulus skin of sufficient strength that elements of a construction can be formed and will maintain the desired configuration even if handled, packaged, and shipped after relatively short cure times, without showing permanent deformation.
- storage stability as defined herein means that the uncured composition maintains its rheology during storage and when cured, the green strength is essentially the same or improved relative to the green strength of the composition prior to storage.
- One objective of this invention is to prepare an alkoxy-functional RTV composition having improved green strength upon curing. Another objective of this invention is to prepare an alkoxy-functional RTV composition having improved storage stability.
- This invention is an alkoxy-functional RTV composition, curable in the presence of moisture, comprising
- each R is independently selected from the group consisting of methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, and isobutyl
- R 1 is selected from the group consisting of methyl and ethyl
- x is 0 or 1;
- each R 4 is independently selected from the group consisting of methyl, ethyl, and vinyl
- each R 5 is independently selected from the group consisting of methyl and ethyl
- z is 1 or 2; with the proviso that components (A), (B), (C), and (D) are added in amounts such that a molar ratio (I) is at least 0.9 and a molar ratio (II) is at least 0.6, where ##EQU1##
- Component (A) comprises polymers comprising on average at least 1.2 alkoxysilyl chain terminations per molecule described by the formula --SiR 1 x (OR) 3-x , where R, R 1 and x are as defined above.
- the polymers may be linear or branched and may be homopolymers, copolymers, or terpolymers.
- the polymers may be a single species or a mixture of different polymers so long as the polymers comprise on average at least 1.2 alkoxysilyl chain terminations per molecule.
- the repeating units of the polymers of Component (A) may include organic units, such as oxyalkylene units, or preferably siloxy units such as described by R 9 s SiO.sub.(4-s)/2, where each R 9 is independently selected from the group consisting of alkyl groups comprising 1 to 6 carbon atoms, phenyl, and fluorinated alkyl groups, and s is 0, 1, or 2.
- alkyl groups described by R 9 include methyl, ethyl, propyl, butyl and hexyl.
- An example of the fluorinated alkyl groups described by R 9 includes 3,3,3-trifluoropropyl.
- the preferred polymers of Component (A) comprise polydiorganosiloxanes having repeating units described by --(R 9 s SiO.sub.(4-s)/2)f --, where R 9 is methyl, s is 2, and f is a value such that Component (A) has a viscosity within a range of about 0.5 to 3000 Pa.s at 25° C. and preferably within a range of about 5 to 150 Pa.s at 25° C.
- the polymers of Component (A) comprise on average at least 1.2 alkoxysilyl chain terminations per molecule described by the formula --SiR 1 x (OR) 3-x , where R, R 1 and x are as defined above.
- R is independently selected from the group consisting of methyl and ethyl, and x is 0.
- a spacer group Z is bonded to the silicon atom of the alkoxysilyl chain termination, where Z is selected from the group consisting of a divalent hydrocarbon radical free of aliphatic unsaturation comprising about 2 to 18 carbon atoms and a combination of divalent hydrocarbon radicals and siloxane segments comprising about 2 to 7 silicon atoms described by ##STR1## where R 9 is as defined above, each G is a divalent hydrocarbon radical free of aliphatic unsaturation comprising about 2 to 18 carbon atoms, and c is a whole number within a range of about 1 to 6.
- Examples of the divalent hydrocarbon radicals describing Z and G include alkylene radicals such as ethylene, methylmethylene, propylene, butylene, pentylene, and hexylene; and arylene radicals including phenylene; with alkylenes being preferred, and in particular ethylene. More preferably, Z is a combination of divalent hydrocarbon radicals and siloxane segments, as described above, where G is an alkylene, preferably, ethylene; R 9 is methyl; and c is 1.
- the polymers of Component (A) are required to have on average at least 1.2 alkoxysilyl chain terminations per molecule, and preferably, the polymers of Component (A) comprise on average at least 1.5 alkoxysilyl chain terminations per molecule. Since the polymers of Component (A) are required to have on average at least 1.2 alkoxysilyl chain terminations per molecule, some polymers may contain other types of chain terminations.
- organosilyl chain terminations include trimethylsilyl, triethylsilyl, vinyldimethylsilyl, and vinylmethylphenylsilyl, with vinyldimethylsilyl being preferred.
- polydiorganosiloxanes useful in this invention as well as crosslinkers, fillers, and other optional ingredients useful in alkoxy-functional RTV silicone sealant compositions are well known in the art and are illustrated by Ceyzeriat et al., U.S. Pat. No. 3,151,099; Brown et al., U.S. Pat. No. 3,161,614; Weyenberg, U.S. Pat. No. 3,175,993 and U.S. Pat. No. 3,334,067; Klosowski et al., U.S. Pat. No. 4,871,827; Kamis et al., U.S. Pat. No. 4,898,910; and Chu et al., U.S. Pat. No. 4,956,435; all of which are hereby incorporated by reference to show alkoxy-functional RTV silicone sealant ingredients and methods of preparing alkoxy-functional RTV silicone sealant compositions.
- Polydiorganosiloxanes within the scope of Component (A), are exemplified by the disclosures of Brown et al., U.S. Pat. No. 3,161,614, and are described, for example, by formula (I) ##STR2## and by mixtures of the polydiorganosiloxanes described by formula (I) and polydiorganosiloxanes described, for example, by formula (II) ##STR3## where R, R 1 , R 2 , R 9 , x, and f are as defined above.
- Preferred polydiorganosiloxanes within the scope of Component (A) include those described by Weyenberg, U.S. Pat No. 3,175,993 and Klosowski et al., U.S. Pat. No. 4,871,827, which are hereby incorporated by reference, and can be described, for example, by formula (III) ##STR4## where R, R 1 , R 9 , Z, x, and f are as described above.
- the more preferred Component (A) polymers useful in this invention are mixtures of the polydiorganosiloxanes described by formula (III) and polydiorganosiloxanes described by Kamis et al., U.S. Pat. No. 4,898,910, which is hereby incorporated by reference, and described, for example, by formula (IV) ##STR5## where R, R 1 , R 9 , Z, x and f are as defined above.
- Component (A) comprises mixtures of polydiorganosiloxanes described by formulas (III) and (IV), typically 40 percent or less of the chain terminations will be organosilyl chain terminations, with preferably less than 25 percent of the chain terminations being organosilyl chain terminations.
- Component (A) also includes organic polymers comprising on average at least 1.2 alkoxysilyl chain terminations per molecule described by --SiR 1 x (OR) 3-x , where R, R 1 , and x are as defined above.
- the organic polymers within the scope of Component (A) may also comprise a spacer group --Z-- bonded to the silicon atom of the alkoxysilyl chain termination, where Z is as defined above.
- One type of organic polymer useful in the invention is the polyoxyalkylene, described by Okawa et al., U.S. Pat. No.
- Component (A) useful in the alkoxy-functional RTV compositions of this invention is dependent on the amounts of other components added so that molar ratios (I) and (II) as described below are met. Typically, however, Component (A) is added in amounts from about 30 to 85 weight percent based on the total weight of the alkoxy-functional RTV composition.
- the alkoxy-functional RTV compositions of the present invention also comprise a tetraalkoxytitanium compound (B) comprising on average greater than 90 mole percent of the alkoxy groups as t-amyloxy groups.
- This tetraalkoxytitanium compound can be a single species or a mixture of different tetraalkoxytitanium compounds, so long as on average Component (B) comprises greater than 90 mole percent of the alkoxy groups as t-amyloxy groups. It is preferred that the tetraalkoxytitanium compound comprise on average at least 98 mole percent of the alkoxy groups as t-amyloxy groups.
- the alkoxy groups substituted on the tetraalkoxytitanium compound which are not t-amyloxy groups can include any alkoxy group having from 1 to 6 carbon atoms. Examples of these groups include methoxy, ethoxy, n-propyloxy, isopropyloxy, n-butoxy, t-butoxy, and hexoxy.
- the tetraalkoxytitanium compounds of this invention may be prepared in different ways.
- the tetraalkoxytitanium compounds can be prepared by reacting tetrachlorotitanium or a tetraalkoxytitanium such as tetraisopropoxytitanium with tertiary-amyl alcohol. These reactions produce hydrochloric acid as a by-product if the tetrachlorotitanium is used; or an alcohol, such as isopropanol, as a by-product, if the tetraalkoxytitanium is used, which byproducts are preferably removed from the reaction medium.
- the starting tetraalkoxytitanium is preferably selected to ensure easy removal of the alcohol byproduct by vacuum devolatilization. Therefore, the alcohol by-product should have a boiling point which permits its easy removal from the reaction mixture without interfering with the preparation of the desired tetraalkoxytitanium compound.
- the boiling points of isopropanol and tertiary-amyl alcohol are 82° C. and 102° C., respectively.
- Reaction of tertiary-amyl alcohol favorably replaces the alkoxy groups on tetraisopropoxytitanium, tetraethoxytitanium, and tetramethoxytitanium to produce a tetraalkoxytitanium containing t-amyloxy groups. These reactions would be continued until on average greater than 90 mole percent of the alkoxy groups on the tetraalkoxytitanium have exchanged with the tertiary-amyl alcohol.
- Component (B) useful in the alkoxy-functional RTV compositions of this invention is dependent on the amounts of other components added so that molar ratios (I) and (II) as described below are met. Typically, however, Component (B) is added in amounts in the range of about 0.1 to 5 weight percent based on the total weight of the alkoxy-functional RTV composition. Preferably, Component (B) is added in amounts in the range of about 1.5 to 3.5 weight percent on the same basis.
- the tetraalkoxytitanium compound may be a single species or a mixture of two or more species.
- the alkoxy-functional RTV compositions of the present invention also comprise a filler (C) having hydroxyl content derived from covalently bonded hydroxyl groups, adsorbed water, or both covalently bonded hydroxyl groups and adsorbed water.
- covalently bonded hydroxyl groups means those hydroxyl groups covalently bonded to the filler which are available for reaction.
- adsorbed water means associated water on the filler surface available for reaction and water from within the filler which becomes available for reaction.
- a particular filler may only have adsorbed water and may not have any covalently bonded hydroxyl groups. However, many fillers have both covalently bonded hydroxyl groups and adsorbed water, for example, untreated fumed silica filler.
- the hydroxyl content of a filler can be altered by drying the filler and/or pretreating the filler with hydrophobing agents such as hexamethyldisilazane. It is preferred to use fillers which have a low hydroxyl content.
- the filler can be selected from those known to be useful in alkoxy-functional RTV sealants.
- the fillers include ground, precipitated, and colloidal calcium carbonates which are untreated or treated with stearate; reinforcing silicas such as fumed silicas, precipitated silicas, and hydrophobed silicas; crushed quartz, ground quartz, alumina, aluminum hydroxide, titanium dioxide, diatomaceous earth, iron oxide, carbon black, and graphite. Fumed silica and calcium carbonate are especially useful and blends of reinforcing fumed silica filler and ground calcium carbonate are preferred.
- the amount of filler useful in the alkoxy-functional RTV compositions generally is that amount of filler which provides the desired properties to the uncured composition such as viscosity, thixotropy, pigmentation, and UV protection.
- the amount of filler also depends upon the cured physical properties desired such as tensile strength, elongation, and durometer.
- the amount of filler useful in the alkoxy-functional RTV compositions of this invention is dependent not only on the above but also on the amounts of other components added, as well as the hydroxyl content of the specific filler used, so that molar ratios (I) and (II) as described below are met. Typically, however, the filler is added in amounts in the range of about 5 to 50 weight percent based on the total weight of the alkoxy-functional RTV composition.
- the filler may be a single species or a mixture of two or more species.
- the alkoxy-functional RTV compositions of the present invention also comprise an alkoxysilane (D) described by formula
- each R 4 is independently selected from the group consisting of methyl, ethyl, and vinyl
- each R 5 is independently selected from the group consisting of methyl and ethyl
- z is 1 or 2.
- useful alkoxysilanes include methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, dimethyldimethoxysilane, vinylmethyldimethoxysilane, dimethyldiethoxysilane, and ethylmethyldiethoxysilane.
- the partial hydrolyzates of these alkoxysilanes can also be used in the present composition.
- Preferred alkoxysilanes include methyltrimethoxysilane and dimethyldimethoxysilane.
- the amount of alkoxysilane useful in the alkoxy-functional RTV compositions of this invention is dependent on the amounts of other components added so that molar ratios (I) and (II) as described below are met. Typically, however, the alkoxysilane is added in amounts in the range of about 0.1 to 10 weight percent based on the total weight of the alkoxy-functional RTV composition, with amounts in the range of about 0.1 to 3 weight percent on the same basis being preferred.
- the alkoxysilane may be a single species or a mixture of two or more species.
- Molar ratio (I) is defined herein as the sum of the moles of tetraalkoxytitanium compound (Component (B)) plus the moles of alkoxysilane (Component (D)) divided by the moles of hydroxyl content in the filler (Component(C)).
- molar ratio (I) is in the range of about 0.9 to 5, and more preferably molar ratio (I) is in the range of about 1 to 2.5.
- both the alkoxysilane and the tetraalkoxytitanium compound are in the numerator of molar ratio (I)
- having a ratio greater than 5 could mean increasing one or both of those components.
- increased amounts of alkoxysilane tends to decrease the development of green strength and increased amounts of the tetraalkoxytitanium compound adds cost to the composition and reduces the hydrolytic stability.
- the hydroxyl content in the filler could also be reduced to decrease the denominator of molar ratio (I), however, it is impractical to reduce the hydroxyl content of the filler below a certain level.
- Molar ratio (II) is defined herein as the moles of tetraalkoxytitanium compound (Component (B)) divided by the sum of the moles of alkoxysilane (Component (D)) plus the moles of alkoxysilyl chain terminations in the polymers (Component (A)).
- molar ratio (II) is in the range of about 0.6 to 2
- more preferably molar ratio (II) is in the range of about 0.65 to 1.
- improved green strength is obtained when molar ratio (II) is above 2, other considerations make these compositions less desirable. For example, increased amounts of the tetraalkoxytitanium compound adds cost to the composition and reduces the hydrolytic stability.
- ingredients which are conventionally used in alkoxy-functional RTV compositions such as adhesion promoters, rheology additives, fungicides, colorants, pigments, and plasticizers, can be added as long as they do not interfere with the rapid development of green strength, either initially or upon storage, or reduce other desired properties.
- organofunctional trialkoxysilanes are used as adhesion promoters and their amounts are such that the moles of organofunctional trialkoxysilane may be significant with respect to the moles of alkoxysilane added, it may be desirable to include the moles of such adhesion promoter as part of the moles of alkoxysilane in determining molar ratios (I) and (II).
- the alkoxy-functional RTV compositions of this invention have improved green strength and storage stability. These results occur when on average greater than 90 mole percent of the alkoxy groups bonded to the tetraalkoxytitanium compound are t-amyloxy groups and molar ratios (I) and (II) are met.
- part or parts by weight (expressed as “pbw”) and viscosities were measured at 25° C.
- Me represents methyl
- AS chain term represents alkoxysilyl chain terminations
- Ot-Am represents tertiary-amyloxy
- Ot-Bu represents tertiary-butoxy
- OiPr represents isopropoxy.
- Polymer a polymer mixture of polydimethylsiloxanes where one type of polymer is described by formula ##STR6## and another type of polymer is described by formula ##STR7## where in the polymer mixture 20 percent of the chain terminations are organosilyl chain terminations and f had an average value such that the polymer mixture's overall viscosity was 60 Pa.s. Some small fraction of a polymer where both chain terminations are organosilyl chain terminations may be present as a by-product from the preparation of the polymers.
- Titanium 1 a mixture of titanium molecules having an average formula Ti(Ot-Am) 3 .92 (OiPr) 0 .08 ; containing at least 98 mole percent -Ot-Am groups
- Titanium 2 Ti(Ot-Bu) 4 ; containing 100 mole percent -Ot-Bu groups
- Titanium 3 a mixture of titanium molecules having an average formula Ti(Ot-Am) 3 .6 (OiPr) 0 .4 ; containing 90 mole percent -Ot-Am groups
- Alkoxysilane 1 methyltrimethoxysilane
- Alkoxysilane 2 dimethyldimethoxysilane
- Silica Filler fumed silica filler having a surface area of 150 m 2 /g and an adsorbed water content of 0.6 weight percent
- CaCO 3 a ground calcium carbonate having an average particle size of 2-3 micrometers, surface treated with stearic acid, and having an adsorbed water content of 0.05 weight percent
- ppt CaCO 3 a precipitated calcium carbonate having a surface area of about 22 m 2 /g, surface treated with stearic acid and having an adsorbed water content of 0.4 weight percent
- Adhesion Promoter a mixture of aminopropyltrimethoxysilane and glycidoxypropyltrimethoxysilane
- Alkoxy-functional RTV sealant compositions were prepared, under conditions to exclude moisture, using the ingredients and procedures described in the following examples. After five days storage at 25° C. and 50% relative humidity, aluminum lap shear joints were constructed and tested as described below. Aluminum panels measuring 2.54 cm ⁇ 7.62 cm were assembled into lap shear joints with a 2.54 cm overlap. The glue line thickness was 0.254 cm. Samples were allowed to cure for 30 minutes by exposure to atmospheric conditions of 25° C. and 50% relative humidity and then the green strength values were measured. The values were measured using an Instron Tensile Tester at a pull rate of 1.27 cm per minute. The values for three lap shear panels were averaged and reported as the green strength for each formulation. Green strength (lap shear) testing following 30 minutes of cure time was repeated after storing the uncured sealant for 1 week at 50° C.
- the extrusion rate was determined by test procedure MIL-S-8802D on the uncured RTV silicone sealant composition by extruding it through a nozzle with a 0.32 cm orifice at 620 KPa pressure and measuring the amount extruded in grams per minute (g/min).
- alkoxy-functional RTV sealant compositions were each prepared, under conditions to exclude moisture, using the ingredients described in Table I.
- the compositions were prepared by first adding alkoxysilane and titanium compound to the polymer, mixing, adding filler, mixing, and drawing a vacuum to remove incorporated air.
- the moles of groups and ingredients were based on 100 grams of the RTV sealant composition and appear in Table I in parenthesis below the weight parts. Molar ratios (I) and (II) as defined in this specification, were determined using the provided mole values.
- the alkoxy-functional RTV sealant compositions were stored in containers sealed to prevent atmospheric moisture from entering. Green strength testing was done as described above and the results are provided in Table I.
- Example 1 shows excellent green strength both initially and after storage at 1 week/50° C. using Titanium 1, a tetraalkoxytitanium compound containing at least 98 mole % Ot-Am groups as compared to the green strength results obtained using Titanium 2 and Titanium 3 which are both outside the scope of this invention.
- RTV sealant compositions were prepared and tested in the same manner as Examples 1-3, the ingredients, their amounts, and the properties measured are provided in Table II. Comparative Examples 4 and 6 illustrate the criticality of the lower end of molar ratios (I) and (II) for improved green strength.
- RTV sealant compositions were prepared and tested in the same manner as Examples 1-3, the ingredients, their amounts, and the properties measured are provided in Table III.
- Examples 8 and 9 show that improved green strength is obtainable using different fillers and
- Example 10 shows that improved green strength is obtainable using an alkoxysilane having 2 alkoxy groups.
- RTV sealant compositions were prepared and tested as described for Examples 1-3, the ingredients, their amounts, and the properties measured are provided in Table IV. Examples 11 and 12 show that improved green strength is still obtainable if the rheology additive or adhesion promoter are removed.
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Abstract
Description
--SiR.sup.1.sub.x (OR).sub.3-x,
R.sup.4.sub.z Si(OR.sup.5).sub.4-z,
R.sup.4.sub.z Si(OR.sup.5).sub.4-z
TABLE I ______________________________________ Use of Different Tetraalkoxytitanium Compounds EXAMPLE INGREDIENT 1 2* 3* ______________________________________ POLYMER, pbw 52.75 52.75 53.00 (moles AS chain term.) (0.00138) (0.00138) (0.00138) TITANIUM 1, pbw 2.00 0.0 0.0 (moles titanium) (0.00505) (0.0) (0.0) TITANIUM 2, pbw 0.0 0.0 1.75 (moles titanium) (0.0) (0.0) (0.00515) TITANIUM 3, pbw 0.0 2.0 0.0 (moles titanium) (0.0) (0.00505) (0.0) ALKOXYSILANE 1, pbw 0.75 0.75 0.75 (moles silane) (0.00551) (0.00551) (0.00551) SILICA FILLER, pbw 3.5 3.5 3.5 (moles OH) (0.00233) (0.00233) (0.00233) CaCO3, pbw 40.0 40.0 40.0 (moles OH) (0.00222) (0.00222) (0.00222) RHEOLOGY ADDITIVE, pbw 0.5 0.5 0.5 ADHESION PROMOTER, pbw 0.5 0.5 0.5 MOLAR RATIO (I) 2.32 2.32** 2.34** MOLAR RATIO (II) 0.73 0.73** 0.75** EXTRUSION RATE (g/min) 81 93 85 GREEN STRENGTH, Pa 7584 5516 4826 (Initial) GREEN STRENGTH, Pa 9653 4137 5516 (1 week/50° C. aging) ______________________________________ *Comparative Example **These values for molar ratio (I) and molar ratio (II) include moles of Titanium 2 and moles of Titanium 3 which were not within the scope of the titanium compound of the present invention.
TABLE II __________________________________________________________________________ Compositions Having Varying Molar Ratios EXAMPLE INGREDIENT 1 4* 5 6* 7 __________________________________________________________________________ POLYMER, pbw 52.75 54.80 47.30 53.40 51.75 (moles AS chain term) (0.00138) (0.00143) (0.00123) (0.00139) (0.00135) TITANIUM 1, pbw 2.00 0.60 5.70 1.00 3.50 (moles titanium) (0.00505) (0.00152) (0.0144) (0.00253) (0.00884) ALKOXYSILANE 1, pbw 0.75 0.10 2.50 1.10 0.25 (moles silane) (0.00551) (0.000735) (0.0184) (0.00809) (0.00184) SILICA FILLER, pbw 3.5 3.5 3.5 3.5 3.5 (moles OH) (0.00233) (0.00233) (0.00233) (0.00233) (0.00233) CaCO3, pbw 40.0 40.0 40.0 40.0 40.0 (moles OH) (0.00222) (0.00222) (0.00222) (0.00222) (0.00222) RHEOLOGY ADDITIVE, pbw 0.5 0.5 0.5 0.5 0.5 ADHESION PROMOTER, pbw 0.5 0.5 0.5 0.5 0.5 MOLAR RATIO (I) 2.32 0.49 7.19 2.33 2.34 MOLAR RATIO (II) 0.73 0.70 0.73 0.27 2.77 EXTRUSION RATE (g/min) 81 46 194 90 63 GREEN STRENGTH, Pa 7584 689 6205 689 17237 (Initial) GREEN STRENGTH, Pa 9653 2068 6895 689 17926 (1 week/50° C. aging) __________________________________________________________________________ *Comparative Example
TABLE III ______________________________________ Affect of Fillers or Alkoxysilane EXAMPLE INGREDIENT 1 8 9 10 ______________________________________ POLYMER, pbw 52.75 88.50 54.50 53.25 (moles AS chain term) (0.00138) (0.00231) (0.00142) (0.00139) TITANIUM 1, pbw 2.00 2.25 3.50 2.00 (moles titanium) (0.00505) (0.00568) (0.00884 (0.00505) ALKOXYSILANE 1, 0.75 0.75 1.50 0.0 pbw (moles silane) (0.00551) (0.00551) (0.0110) (0.0) ALKOXYSILANE 2, 0.0 0.0 0.0 0.66 pbw (moles silane) (0.0) (0.0) (0.0) (0.00550) SILICA FILLER, pbw 3.5 7.0 0.0 3.5 (moles OH) (0.00233) (0.00467) (0.0) (0.00233) CaCO3, pbw 40.0 0.0 0.0 40.0 (moles OH) (0.00222) (0.0) (0.0) (0.00222) ppt. CaCO3, pbw 0.0 0.0 40.0 0.0 (moles OH) (0.0) (0.0) (0.0178) (0.0) RHEOLOGY 0.5 1.0 0.0 0.5 ADDITIVE, pbw ADHESION 0.5 0.5 0.5 0.5 PROMOTER, pbw MOLAR RATIO (I) 2.32 2.40 1.12 2.32 MOLAR RATIO (II) 0.73 0.73 0.71 0.73 EXTRUSION RATE 81 100 93 56 (g/min) GREEN STRENGTH, Pa 7584 10342 8274 12411 (Initial) GREEN STRENGTH, Pa 9653 10342 8963 10342 (1 week/50° C. aging) ______________________________________
TABLE IV ______________________________________ Effect of Rheology Additive or Adhesion Promoter EXAMPLE INGREDIENT 1 11 12 ______________________________________ POLYMER, pbw 52.75 53.25 53.25 (moles AS chain term) (0.00138) (0.00139) (0.00139) TITANIUM 1, pbw 2.00 2.00 2.00 (moles titanium) (0.00505) (0.00505) (0.00505) ALKOXYSILANE 1, pbw 0.75 0.75 0.75 (moles silane) (0.00551) (0.00551) (0.00551) SILICA FILLER, pbw 3.5 3.5 3.5 (moles OH) (0.00233) (0.00233) (0.00233) CaCO3, pbw 40.0 40.0 40.0 (moles OH) (0.00222) (0.00222) (0.00222) RHEOLOGY ADDITIVE, pbw 0.5 0.5 0.0 ADHESION PROMOTER, pbw 0.5 0.0 0.5 MOLAR RATIO (I) 2.32 2.32 2.32 MOLAR RATIO (II) 0.73 0.73 0.73 EXTRUSION RATE (g/min) 81 103 90 GREEN STRENGTH, Pa (initial) 7584 9653 8274 GREEN STRENGTH, Pa 9653 11721 8274 (1 week/50° C. aging) ______________________________________
Claims (24)
--SiR.sup.1.sub.x (OR).sub.3-x,
R.sup.4.sub.z Si(OR.sup.5).sub.4-z,
--SiR.sup.1.sub.x (OR).sub.3-x,
R.sup.4.sub.z Si(OR.sup.5).sub.4-z,
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Also Published As
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EP0905194A3 (en) | 2000-02-02 |
JPH11181287A (en) | 1999-07-06 |
EP0905194A2 (en) | 1999-03-31 |
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